反应详情

To a solution of a sample of the previous residue (160 mg) in dimethylformamide (2.5 mL) was added N,N-diisopropylethylamine (181 μL), 4-methyl-4-methyldisulfanyl-pentanoic acid (158 mg), N,N′-diisopropyl-carbodiimide (88 μL) and 1-hydroxybenzotriazole hydrate (15 mg). After 15 h at room temperature, solids were filtered off and the dimethylformamide solution was injected for HPLC purification according to method F. The appropriate fractions were combined and concentrated by freeze-drying to afford 4-(3-[4-(4-methyl-4-methyldisulfanyl-pentanoyl)-piperazin-1-yl]-propyl)-2,6-bis-(hydroxymethyl)-pyridine (105 mg):

1. filtrationsolids were filtered off
2. customthe dimethylformamide solution was injected for HPLC purification
3. concentrationconcentrated
4. customby freeze-drying